Porous liquid gas chromatography chiral column for splitting racemic compound
A gas chromatography and chiral column technology, applied in the field of capillary gas chromatography chiral separation, to achieve the effects of excellent chiral separation performance, good stability and easy availability of raw materials
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Embodiment 1
[0022] (1) Preparation of chiral MOF D-his-ZIF-8 nanocrystals: D-histidine (0.1 g, 0.64 mmol) was added to methanol / water (45 mL / 8 mL, V / V) solution, and then the Zn(NO 3 ) 2 ·6H 2 O (0.36 g, 1.4 mmol) and 2-methylimidazole (0.4 g, 4.9 mmol) were respectively dissolved in D-histidine solution; then, Zn(NO 3 ) 2 ·6H 2 The O solution was added to the 2-methylimidazole solution, stirred at room temperature for one day, the product was collected by centrifugation, and washed three times with methanol to obtain D-his-ZIF-8 nanocrystals;
[0023] (2) Chiral Porous Liquid D-his-ZIF-8-[Bpy][NTf 2 ]: Add wet D-his-ZIF-8 (20 mg) nanocrystals to 1 mL of [Bpy][NTf 2 ] ionic liquid, and stirred for 1 h at 100 °C under vacuum to remove methanol to obtain a chiral porous liquid D-his-ZIF-8-[Bpy][NTf 2 ]; Synthesized chiral porous liquid D-his-ZIF-8-[Bpy][NTf 2 ] Able to remain stable for months without settling and has a Tyndall effect;
[0024] (3) Roughening treatment of the inner...
Embodiment 2
[0027] The capillary chiral column prepared in Example 1 was used to perform chromatographic resolution tests on different types of racemic compounds to investigate their resolution effects. For the resolved chromatogram see image 3 . image 3 The chiral compounds resolved in the middle are: (a) n-butyl glycidyl ether, column temperature 175 °C; (b) styrene oxide, column temperature 160 °C; (c) 3-chloro-2-butanone, column temperature temperature 115℃; (d) methyl 2-bromobutyrate, column temperature 155℃; (e) 2-pentanol, column temperature 120℃; (f) 2-pinene, column temperature 150℃; (g) 2 -Methyltetrahydrofuran-3-one, column temperature 130°C; (h) 2-butanol, column temperature 110°C; (i) 1,2-dichloropropane, column temperature 100°C. Other chromatographic conditions: high-purity nitrogen as carrier gas, inlet temperature 250°C, and detector temperature 250°C.
[0028] Depend on image 3 It can be seen that the chiral porous liquid capillary gas chromatography column prepar...
Embodiment 3
[0030] In order to study the stability and reproducibility of the capillary chiral column prepared in Example 1, after using the column for a period of time (1 month, 2 months, 3 months, 6 months), The alcohol is separated, and its separation chromatogram is shown in the attached image 3 . Chromatographic conditions: high-purity nitrogen as carrier gas, inlet temperature 250°C, detector temperature 250°C, split ratio 40:1, column temperature 125°C.
[0031] Depend on image 3 It can be seen that the capillary chiral column prepared in Example 1 has no obvious change in the splitting effect of 2-butanol after 1 month, 2 months, 3 months and 6 months of use and the beginning of use, indicating that The chromatographic column of the invention has good stability and reproducibility, and has good practical application prospects.
[0032] Table 1 chromatographic column of the present invention to the results of resolution of some racemic compounds
[0033]
[0034] Chromatog...
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